CN1904584A - Fast analysis method of ammonium perchlorate particle size in solid propellant - Google Patents
Fast analysis method of ammonium perchlorate particle size in solid propellant Download PDFInfo
- Publication number
- CN1904584A CN1904584A CN 200610010323 CN200610010323A CN1904584A CN 1904584 A CN1904584 A CN 1904584A CN 200610010323 CN200610010323 CN 200610010323 CN 200610010323 A CN200610010323 A CN 200610010323A CN 1904584 A CN1904584 A CN 1904584A
- Authority
- CN
- China
- Prior art keywords
- ammonium perchlorate
- sample
- particle size
- solid propellant
- rapid analysis
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Landscapes
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The invention relates to a rapid analysis method for granularity of ammonium perchlorate in solid propellant. It includes the following steps: collecting ammonium perchlorate sample of purity over 99.5% by screen method; gathering sample spectrum and building database; selecting representative sample by math method and taking preprocess, building standard sample model by using the wave length information of amino between first level double frequency absorption peak of 6463cm-1 and combining frequency absorption peak of 4680cm-1; comparing the granularity of pre-testing to that of sample to judge whether it is qualified; if it is not qualified, judging whether it is out-drop point; if it is out-drop point, taking second judgment; if not, returning to the first step. The invention is easy to operate and has rapid analyzing speed.
Description
Technical field
The present invention relates to a kind of ammonium perchlorate particle size's analytical approach.
Background technology
At present sieve classification mensuration and microscope micrometry were mainly adopted in the granulometry of solid propellant, no matter adopt above-mentioned which kind of method, all exist operation steps more loaded down with trivial details, measuring needs a large amount of samples, the experimental data that provides often all lags behind production run, causes production process monitoring not exclusively and go wrong and can not in time find.To improve in the solid propellant fast detecting of quality imperative for this reason.
Preparation with oxygenant in solid propellant is prepared is the most complicated, and oxygenant adopts ammonium perchlorate and will be by screening strict control particle size and distribution thereof more, because the flowability of the granularity of ammonium perchlorate medicine slurry during to the combustion speed characteristic of propellant, density, mechanical property and cast all has remarkable influence.Determine correct granule size and shape, become the main task in the oxidant preparing process.Therefore production technology must be accompanied by the strict quality program, and is extremely important to ammonium perchlorate particle size's detection.
Summary of the invention
The object of the present invention is to provide the rapid analysis of ammonium perchlorate particle size in a kind of solid propellant, this method can solve and adopt sieve method and microscope micrometry to measure the ammonium perchlorate particle size, there is complex operation step, measuring needs a large amount of samples, the experimental data that provides often all lags behind production run, causes the problem that production process monitoring is incomplete and go wrong and can not in time find.
The present invention is finished by following steps: adopting traditional method for sieving to collect purity is ammonium perchlorate sample more than 99.5%, sets up sample library 001; Is 12000cm with the Fourier transform near infrared spectrum analyser at wavelength
-1～4000cm
-1Collected specimens spectrum in the scope is set up sample spectra picture library 002; Select representative sample 003 with mathematical method; Representational sample is carried out pre-service, is 12000cm to pretreated representative sample at wavelength with chemometrics method again
-1～4000cm
-1Carry out information extraction, the optimization of collection of illustrative plates in the scope, utilize amino to be 6463cm at wavelength
-1One-level frequency multiplication absorption peak and wavelength be 4680cm
-1Sum of fundamental frequencies absorption peak information set up standard model model 004; The granularity of the granularity of standard model model prediction and the sample that obtains by traditional method for sieving is compared 005; Criterion instance model whether qualified 006; If judged result is qualified, then the standard model that is detected is certified products 007; If judged result is defective, continue to judge that whether the standard model that is detected is for out-of-bounds putting 008; If judged result is a point out-of-bounds, add and out-of-bounds put 009, be back to 004 step again; If judged result is then returned 001 step for not being point out-of-bounds.
The present invention has following beneficial effect: one, method of the present invention is applicable to behind the off-line granularity of ammonium perchlorate in the fast detecting solid propellant, analytic sample is finished within 30s, there is not destructiveness, safety, environmental protection, personnel are safe from harm, analyze a large amount of samples save time, laborsaving, save cost, processing ease.Two, utilize the Fourier transform near infrared spectrum analyser can react the variation of every quality index of ammonium perchlorate sample fast, in real time, thereby guarantee the quality of solid propellant, practical large-scale is produced directive significance very much.Three, simple, the operation easily of method of the present invention need not a large amount of samples during measurement, the experimental data and the production run that provide are synchronous, can monitor in real time in process of production, and can in time scent a hidden danger.
Description of drawings
Fig. 1 is the process step figure of the inventive method, Fig. 2 is the granularity of the standard model model prediction in the embodiment two and the two correlogram of the granularity of the sample that obtains by traditional method for sieving, Fig. 3 is the correlogram of granularity between the two of the granularity of the standard model model prediction in the embodiment three and the sample that obtains by traditional method for sieving, and Fig. 4 is an ammonium perchlorate near infrared light spectrogram.
Embodiment
Embodiment one: present embodiment is described in conjunction with Fig. 1, ammonium perchlorate particle size's rapid analysis is finished by following steps in the solid propellant of present embodiment: adopting traditional method for sieving to collect purity is ammonium perchlorate sample more than 99.5%, sets up sample library 001; Is 12000cm with the Fourier transform near infrared spectrum analyser at wavelength
-1～4000cm
-1Collected specimens spectrum in the scope is set up sample spectra picture library 002; Select representative sample 003 with mathematical method; Representational sample is carried out pre-service, is 12000cm to pretreated representative sample at wavelength with chemometrics method again
-1～4000cm
-1Carry out information extraction, the optimization of collection of illustrative plates in the scope, utilize amino to be 6463cm at wavelength
-1One-level frequency multiplication absorption peak and wavelength be 4680cm
-1Sum of fundamental frequencies absorption peak information set up standard model model 004; The granularity of the granularity of standard model model prediction and the sample that obtains by traditional method for sieving is compared 005; Criterion instance model whether qualified 006; If judged result is qualified, then the standard model that is detected is certified products 007; If judged result is defective, continue to judge that whether the standard model that is detected is for out-of-bounds putting 008; If judged result is a point out-of-bounds, add and out-of-bounds put 009, be back to 004 step again; If judged result is then returned 001 step for not being point out-of-bounds.Ammonium perchlorate used in the present embodiment is provided by Dalian Potassium Chlorate Plant.
Present embodiment is in 003 step, and described mathematical method is selected from a kind of in clustering procedure, major component factorization method or the gridding method.
Present embodiment is in 004 step, and described preprocess method is selected from a kind of in straight line deduction, vector normalization, minimax normalization, polynary scatter correction, first order derivative, second derivative, linear compensation minusing or the first order derivative method; Described chemometrics method be selected from partial least square method, principal component analysis, progressively return or the artificial neural network method in a kind of.Because instrument, sample background or other factor affecting, the skew or the drift phenomenon that often occur spectrogram in the near-infrared spectrum analysis, to such an extent as to eliminate of the influence of various non-target factors to spectrum in order to weaken, make spectroscopic data fully reflect change information, improve the quality of calibration model and the accuracy that unknown sample predicts the outcome, the original spectrum that collects is carried out pre-service.
Ammonium perchlorate mainly is amino absorption in the absorption of near infrared region, and characteristic wavelength is 6463cm
-1One-level frequency multiplication absorption peak and 4680cm
-1Sum of fundamental frequencies absorption peak (referring to accompanying drawing 4).
Present embodiment is in 002 step, described Fourier transform near infrared spectrum analyser adopts integrating sphere irreflexive MPA Fourier transform near infrared spectrum analyser or the irreflexive MPA Fourier transform near infrared spectrum of fibre-optical probe analyser, more than two analysers make by Germany (Bruker), detecting device in the Fourier transform near infrared spectrum analyser is elected the InGeAs detecting device as, wherein a kind of of PbS detecting device and InAs detecting device, with the PbS detecting device is best, but utilizes the on-line monitoring of the irreflexive MPA Fourier transform near infrared spectrum of fibre-optical probe analyser.Method of the present invention not only can be measured the granularity of ammonium perchlorate, also can measure the molecular weight of the middle size-grade distribution of oxygenant (ammonium perchlorate) and moisture and bonding agent, the indexs such as degree, ageing properties and combustion speed of curing.
Embodiment two: the traditional method for sieving collection purity of employing is 99.5% aciculiform ammonium perchlorate sample in 001 step of present embodiment, and used sieve number is 40 orders～130 orders, is divided into different stage, demarcates screen overflow with the order number of screen cloth; Adopt the irreflexive MPA Fourier transform near infrared spectrum of integrating sphere analyser in 002 step, resolution is 8cm
-1, scanning times is that 64 times, the diameter of sample spinner are 50mm.Other step is identical with embodiment one.
In the present embodiment, the related coefficient between the granularity of the granularity of standard model model prediction and the sample that obtains by traditional method for sieving is that the slope of R=0.9988, straight line is 0.9915, intercept is 0.716, the coefficient of determination of model is 99.38 (referring to accompanying drawings 2).
Embodiment three: it is 99.8% spherical ammonium perchlorate sample that present embodiment adopts traditional method for sieving to collect purity in 001 step, and used sieve number is 50 orders～160 orders, is divided into different stage, demarcates screen overflow with the order number of screen cloth.Other step is identical with embodiment one.
In the present embodiment, the related coefficient between the granularity of the granularity of standard model model prediction and the sample that obtains by traditional method for sieving is that the slope of R=0.999, straight line is 0.999, intercept is 0.482, the coefficient of determination of model is 99.04 (referring to accompanying drawings 3).
Claims (10)
1, ammonium perchlorate particle size's rapid analysis in a kind of solid propellant is characterized in that it is finished by following steps: adopting traditional method for sieving to collect purity is ammonium perchlorate sample more than 99.5%, sets up sample library (001); Is 12000cm with the Fourier transform near infrared spectrum analyser at wavelength
-1～4000cm
-1Collected specimens spectrum in the scope is set up sample spectra picture library (002); Select representative sample (003) with mathematical method; Representational sample is carried out pre-service, is 12000cm to pretreated representative sample at wavelength with chemometrics method again
-1～4000cm
-1Carry out information extraction, the optimization of collection of illustrative plates in the scope, utilize amino to be 6463cm at wavelength
-1One-level frequency multiplication absorption peak and wavelength be 4680cm
-1Sum of fundamental frequencies absorption peak information set up standard model model (004); The granularity of the granularity of standard model model prediction and the sample that obtains by traditional method for sieving is compared (005); Whether the criterion instance model qualified (006); If judged result is qualified, then the standard model that is detected is certified products (007); If judged result is defective, continue to judge that whether the standard model that detected is point (008) out-of-bounds; If judged result is a point out-of-bounds, add out-of-bounds point (009), be back to 004 step again; If judged result is then returned 001 step for not being point out-of-bounds.
2, ammonium perchlorate particle size's rapid analysis in the solid propellant according to claim 1, it is characterized in that in 001 step adopting traditional method for sieving to collect purity is 99.5% aciculiform ammonium perchlorate sample.
3, ammonium perchlorate particle size's rapid analysis in the solid propellant according to claim 1, it is characterized in that in 001 step adopting traditional method for sieving to collect purity is 99.8% spherical ammonium perchlorate sample.
4, ammonium perchlorate particle size's rapid analysis in the solid propellant according to claim 1 is characterized in that adopting in 002 step integrating sphere irreflexive MPA Fourier transform near infrared spectrum analyser or the irreflexive MPA Fourier transform near infrared spectrum of fibre-optical probe analyser.
5, ammonium perchlorate particle size's rapid analysis in the solid propellant according to claim 1 is characterized in that the mathematical method described in 003 step is selected from a kind of in clustering procedure, major component factorization method or the gridding method.
6, ammonium perchlorate particle size's rapid analysis in a kind of solid propellant according to claim 1 is characterized in that the preprocess method described in 004 step is selected from a kind of in straight line deduction, vector normalization, minimax normalization, polynary scatter correction, first order derivative, second derivative, linear compensation minusing or the first order derivative method.
7, ammonium perchlorate particle size's rapid analysis in a kind of solid propellant according to claim 1, it is characterized in that the chemometrics method described in 004 step be selected from partial least square method, principal component analysis, progressively return or the artificial neural network method in a kind of.
8, ammonium perchlorate particle size's rapid analysis in the solid propellant according to claim 1 is characterized in that sieve number used in 001 step is 40 orders～160 orders.
9, ammonium perchlorate particle size's rapid analysis in the solid propellant according to claim 1 is characterized in that sieve number used in 001 step is 40 orders～130 orders.
10, ammonium perchlorate particle size's rapid analysis in the solid propellant according to claim 1 is characterized in that sieve number used in 001 step is 50 orders～160 orders.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100103234A CN100557413C (en) | 2006-07-26 | 2006-07-26 | Ammonium perchlorate particle size's rapid analysis in the solid propellant |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100103234A CN100557413C (en) | 2006-07-26 | 2006-07-26 | Ammonium perchlorate particle size's rapid analysis in the solid propellant |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1904584A true CN1904584A (en) | 2007-01-31 |
| CN100557413C CN100557413C (en) | 2009-11-04 |
Family
ID=37673889
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006100103234A Expired - Fee Related CN100557413C (en) | 2006-07-26 | 2006-07-26 | Ammonium perchlorate particle size's rapid analysis in the solid propellant |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100557413C (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103499551A (en) * | 2013-09-25 | 2014-01-08 | 武汉大学 | Method for identifying aging degree of bonding interface of binders |
| CN103792166A (en) * | 2014-01-22 | 2014-05-14 | 西安航天化学动力厂 | Method for measuring granularity of spherical ammonium perchlorate |
| CN105092436A (en) * | 2015-07-31 | 2015-11-25 | 中国石油天然气股份有限公司 | Sediment particle size spectrum analysis method and device |
| CN106018333A (en) * | 2016-07-29 | 2016-10-12 | 西安近代化学研究所 | Rapid prediction method for stable stage of stacked biradical propellant powder |
| CN106093292A (en) * | 2016-07-29 | 2016-11-09 | 西安近代化学研究所 | A kind of NEPE propellant loading safe storage life predictor method |
| CN106290232A (en) * | 2016-07-29 | 2017-01-04 | 西安近代化学研究所 | Pile up storage single-base gun propellant safe storage life predictor method |
| CN110308109A (en) * | 2019-05-05 | 2019-10-08 | 湖北省农业科学院农业质量标准与检测技术研究所 | A method of perchlorate content range in tealeaves is differentiated based near infrared spectrum |
-
2006
- 2006-07-26 CN CNB2006100103234A patent/CN100557413C/en not_active Expired - Fee Related
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103499551A (en) * | 2013-09-25 | 2014-01-08 | 武汉大学 | Method for identifying aging degree of bonding interface of binders |
| CN103792166A (en) * | 2014-01-22 | 2014-05-14 | 西安航天化学动力厂 | Method for measuring granularity of spherical ammonium perchlorate |
| CN103792166B (en) * | 2014-01-22 | 2016-06-01 | 西安航天化学动力厂 | A kind of method measuring spherical ammonium perchlorate particle size |
| CN105092436A (en) * | 2015-07-31 | 2015-11-25 | 中国石油天然气股份有限公司 | Sediment particle size spectrum analysis method and device |
| CN105092436B (en) * | 2015-07-31 | 2018-01-05 | 中国石油天然气股份有限公司 | A kind of grain size of sediment spectroscopic analysis methods and device |
| CN106018333A (en) * | 2016-07-29 | 2016-10-12 | 西安近代化学研究所 | Rapid prediction method for stable stage of stacked biradical propellant powder |
| CN106093292A (en) * | 2016-07-29 | 2016-11-09 | 西安近代化学研究所 | A kind of NEPE propellant loading safe storage life predictor method |
| CN106290232A (en) * | 2016-07-29 | 2017-01-04 | 西安近代化学研究所 | Pile up storage single-base gun propellant safe storage life predictor method |
| CN106093292B (en) * | 2016-07-29 | 2017-12-22 | 西安近代化学研究所 | A kind of NEPE propellant loadings safe storage life predictor method |
| CN106018333B (en) * | 2016-07-29 | 2018-10-12 | 西安近代化学研究所 | Accumulate double-base propellant ultimate stage rapid Estimation method |
| CN106290232B (en) * | 2016-07-29 | 2019-03-08 | 西安近代化学研究所 | Accumulation storage single-base gun propellant safe storage life predictor method |
| CN110308109A (en) * | 2019-05-05 | 2019-10-08 | 湖北省农业科学院农业质量标准与检测技术研究所 | A method of perchlorate content range in tealeaves is differentiated based near infrared spectrum |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100557413C (en) | 2009-11-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100557413C (en) | Ammonium perchlorate particle size's rapid analysis in the solid propellant | |
| CN104062257B (en) | A kind of based on the method for general flavone content near infrared ray solution | |
| CN108519348A (en) | Licorice medicinal materials Near-Infrared Quantitative Analysis model and detection method and standard | |
| CN104897607A (en) | Food modeling and rapid detecting integration method and system adopting portable NIRS (near infrared spectroscopy) | |
| CN101413885A (en) | Near-infrared spectrum method for rapidly quantifying honey quality | |
| CN103033486B (en) | Method for near infrared spectrum monitoring of quality of pericarpium citri reticulatae and citrus chachiensis hortorum medicinal materials | |
| CN102590129B (en) | Method for detecting content of amino acid in peanuts by near infrared method | |
| CN104062258B (en) | Method for rapid determination of soluble solids in compound ass-hide glue pulp by near infrared spectroscopy | |
| CN103091274B (en) | The method of near-infrared diffuse-reflectance spectroscopic assay Radix Salviae Miltiorrhizae for injection Polyphenol Acids moisture | |
| CN101961360A (en) | Near infrared spectrum identification method for pseudo-ginseng | |
| CN106932360A (en) | Portable near infrared spectrum food science literature and modeling integral system and method | |
| CN102914596B (en) | Method for rapidly determining PienTzeHuang quality by using near-infrared spectroscopy | |
| CN103487395A (en) | Quick multi-index detection method for Paris polyphylla medicinal materials | |
| CN102243170A (en) | Method for identifying production place of dwarf lilyturf root by using near infrared spectrum technology | |
| CN104062259A (en) | Method for rapid determination of total saponin content in compound ass-hide glue pulp by near infrared spectroscopy | |
| CN102937575B (en) | Watermelon sugar degree rapid modeling method based on secondary spectrum recombination | |
| CN103411895B (en) | Pseudo-near infrared spectrum identification method mixed by pearl powder | |
| CN105092436A (en) | Sediment particle size spectrum analysis method and device | |
| CN109324014A (en) | A kind of adaptive oil property near-infrared method for quick predicting | |
| CN104730004A (en) | Textile fiber identification method based on ultraviolet diffuse reflectance spectrum | |
| CN104132720A (en) | Method for quickly detecting tablet weight of medicine tablets through near infrared spectroscopy | |
| CN101310738B (en) | Intermediate infrared spectrum polycomponent quantitative analysis method of traditional Chinese medicine extract | |
| CN101701911A (en) | Method for detecting content of reducing sugar in fermentation materials | |
| CN104596979A (en) | Method for measuring cellulose of reconstituted tobacco by virtue of near infrared reflectance spectroscopy technique | |
| CN104596975A (en) | Method for measuring lignin of reconstituted tobacco by paper-making process by virtue of near infrared reflectance spectroscopy technique |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20091104 Termination date: 20210726 |